反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]=1.[Cl:9][C:10]1[CH:11]=[C:12]([C:17]([C:30]([F:33])([F:32])[F:31])=[CH:18][C:19]([C:21]2[CH:29]=[CH:28][C:24]([C:25](Cl)=[O:26])=[CH:23][CH:22]=2)=[O:20])[CH:13]=[C:14]([Cl:16])[CH:15]=1.O>N1C=CC=CC=1>[Cl:8][C:5]1[CH:4]=[N:3][C:2]([NH:1][C:25](=[O:26])[C:24]2[CH:28]=[CH:29][C:21]([C:19](=[O:20])[CH:18]=[C:17]([C:12]3[CH:11]=[C:10]([Cl:9])[CH:15]=[C:14]([Cl:16])[CH:13]=3)[C:30]([F:33])([F:31])[F:32])=[CH:22][CH:23]=2)=[N:7][CH:6]=1参加物
実験手順
To a solution of 0.5 g of 2-amino-5-chloropyrimidine in 20 mL of pyridine, 0.5 g of 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid chloride was poured at room temperature and the mixture was stirred for 2.5 hours. After that, water was added to the reaction solution that was extracted with ethyl acetate, an organic layer was washed with water and diluted hydrochloric acid and then dehydrated and dried with saturated saline followed by anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resulting residue was purified using silica gel column chromatography that was eluted with ethyl acetate-hexane (5:2) followed by crystallization from a mixed solvent of hexane and a small amount of ethyl acetate to obtain 0.31 g of aimed product as white solid.
後処理
- extractionwas extracted with ethyl acetate
- washan organic layer was washed with water and diluted hydrochloric acid
- customdried with saturated saline
- distillationthe solvent was distilled off under reduced pressure
- customThe resulting residue was purified
- washwas eluted with ethyl acetate-hexane (5:2)
- customfollowed by crystallization from a mixed solvent of hexane
出典と根拠
- ORDレコード
- ord-936156af533845649de82c1a29311ee4
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07700808B2
関連ノート
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